A method for the determination of 12 synthetic food dyes (Amaranth, Erythrosine, Allura Red AC, New Coccine, Phloxine, Rose Bengal, Acid Red, Tartrazine, Sunset Yellow FCF, Fast Green FCF, Brilliant Blue FCF, Indigo Carmine) in food was developed using capillary electrophoresis (CE) with photodiode array detection.The dyes were extracted with water and 0.5 ammonia-ethanol (1 : 1) mixture, and cleaned up using solid-phase extraction (Sep-Pak Plus tC18). The dyes were eluted with methanol from the cartridge. The dyes were separated by CE on a bubble cell fused-silica capillary (72 cm to the detector, 75 mm i.d.) using 20 acetonitrile in a mixture of 10 mmol/L potassium phosphate, monobasic and 5 mmol/L sodium carbonate (pH 10.0) as the running bu#er. Identifications of the dyes were performed on the basis of the migration time and the absorbance spectrum of each peak. The coe$cients of variation of the migration times and the peak areas were 0.28ῌ0.62 and 1.84ῌ 4.30, respectively (n5). The identification limits using the absorbance spectra of the dyes were 10 mg/mL for Brilliant Blue FCF and Fast Green FCF, and 5 mg/mL for the other 10 dyes. The recoveries of the 12 dyes from pickles, soft drinks and candies at the level of 10 mg/g were 70.0ῌ 101.5. The method was applied to the analysis of dyes in foods. The dyes detected by CE were in agreement with those detected by paper chromatography.
Azodicarbonamide ADA is used in some countries as a flour bleaching agent and a dough conditioner. However, ADA is prohibited for use as a food additive in Japan. Therefore, it is necessary to establish an efficient and sensitive method to determine ADA in wheat flour. A simple and practical procedure to analyze ADA in wheat flour and prepared flour mixes was developed. ADA was extracted from samples by ultrasonication with acetone. ADA in the solution was derivatized with triphenylphosphine TPP . The ADA-TPP derivative was concentrated and cleaned up using a reversed-phase solid-phase extraction cartridge, and the ADA-TPP derivative was analyzed using HPLC for determination and LC-MS/MS for identification. Good linearity was achieved over the concentration range of 0.25-100 ppm ADA in wheat flour and prepared flour mixes. The mean recoveries from wheat flour and prepared flour mixes fortified at the levels of 1 and 10 ppm ranged from 86.9 to 101.0 , and the coefficients of variation ranged from 1.9 to 3.4 .
A method for the determination of Cinchona extract (whose main components are the alkaloids cinchonine, cinchonidine, quinidine, and quinine) in beverages by liquid chromatography was developed. A beverage with an alcohol content of more than 10% was loaded onto an OASIS HLB solid-phase extraction cartridge, after it was adjusted to pH 10 with 28% ammonium hydroxide. Other beverages were centrifuged at 4000 rpm for 5 min, and the supernatant was loaded onto the cartridge. The cartridge was washed with water followed by 15% methanol, and the Cinchona alkaloids were eluted with methanol. The Cinchona alkaloids in the eluate were chromatographed on an L-column ODS (4.6 mm id × 150 mm) with methanol and 20 mmol/L potassium dihydrogen phosphate (3 + 7) as the mobile phase. Cinchona alkaloids were monitored with an ultraviolet (UV) detector at 230 nm, and with a fluorescence detector at 405 nm for cinchonine and cinchonidine and 450 nm for quinidine and quinine (excitation at 235 nm). The calibration curves for Cinchona alkaloids with the UV detector showed good linearity in the range of 2400 μg/mL. The detection limit of each Cinchona alkaloid, taken to be the concentration at which the absorption spectrum could be identified, was 2 μg/mL. The recovery of Cinchona alkaloids added at a level of 100 μg/g to various kinds of beverages was 87.6-96.5%, and the coefficients of variation were less than 3.3%. A number of beverage samples, some labeled to contain bitter substances, were analyzed by the proposed method. Quinine was detected in 2 samples of carbonated beverage.
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